Solution multinuclear (<sup>31</sup>P,<sup>111</sup>Cd,<sup>77</sup>Se) magnetic resonance studies of cadmium complexes of heterocyclic aromatic thiones and the structure of [tetrakis(2(1<i>H</i>)-pyridinethione)cadmium] nitrate, [Cd(C<sub>5</sub>H<sub>5</sub>NS)<sub>4</sub>](NO<sub>3</sub>)<sub>2</sub>
Why this work is in the frame
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Bibliographic record
Abstract
The complex salts CdL 4 (O 3 SCF 3 ) 2 (L = 2(1H)-pyridinethione (Py2SH), 4(1H)-pyridinethione (Py4SH), or 2(1H)-quinolinethione (Q2SH)) have been synthesized by the stoichiometric reaction of Cd(O 3 SCF 3 ) 2 and the appropriate thione. Both ambient-temperature 13 C and reduced-temperature 111 Cd NMR of CdL 4 (O 3 SCF 3 ) 2 in solution are consistent with L being bound through sulfur. Reduced-temperature NMR ( 31 P, 77 Se, 111 Cd, as appropriate) of mixtures of CdL 4 (O 3 SCF 3 ) 2 and Cd(EPCy 3 ) 4 (O 3 SCF 3 ) 2 (E = Se, Cy = c-C 6 H 11 ) and of Cd(EPCy 3 ) 4 (O 3 SCF 3 ) 2 (E = S, Se) and L in solution provides evidence for various [CdL n (EPCy 3 ) 4- n ] 2+ . Similarly, reduced-temperature metal NMR of [CdL 4 ] 2+ and [CdL' 4 ] 2+ (L, L' = Py2SH, Py4SH, Q2SH; L not equal L') in solution shows the formation of [CdL n L' 4- n ] 2+ . Thus it has been demonstrated that at reduced temperature [CdL 4 ] 2+ is intact in solution and exchange of L is slow on the timescale of the metal chemical shift differences. From the NMR studies of Cd(EPCy 3 ) 4 (O 3 SCF 3 ) 2 (E = S, Se):L mixtures, the binding preferences are found to be L > EPCy 3 in solution. Similarly, from the reduced temperature metal NMR spectra of mixtures where L and L' compete for Cd(II) in solution, the binding preferences are Py4SH > Py2SH > Q2SH. The structure of Cd(Py2SH) 4 (NO 3 ) 2 (4) has been determined by single crystal X-ray analysis. Colorless crystals of 4 are tetragonal, I4(1)/acd with 8 molecules per unit cell of dimensions a = 18.660(3), c = 15.215(3) Å. The structure is comprised of recognizable NO 3 - anions and [Cd(Py2SH) 4 ] 2+ cations. In the cations, which have S 4 symmetry, the ligands are S-bound. A network of NH···O hydrogen bonds links the cations and anions.Key words: aromatic heterocyclic thiones, cadmium complexes, phosphine chalcogenides, 111 Cd, 31 P, 77 Se NMR, X-ray crystallography.
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Full frame distilled prediction
Teacher imitationNot calibrated prevalence, not ground truth. Human validation pending. Learned from the 10,348 direct Codex labels and 10,348 direct Gemma labels. Candidate is the union of thresholded teacher heads; consensus is their intersection. These outputs are machine_predicted_unvalidated and are not human labels or direct frontier model labels.
Codex and Gemma teacher scores by category
| Category | Codex | Gemma |
|---|---|---|
| Metaresearch | 0.002 | 0.002 |
| Meta-epidemiology (narrow) | 0.002 | 0.002 |
| Meta-epidemiology (broad) | 0.004 | 0.001 |
| Bibliometrics | 0.001 | 0.002 |
| Science and technology studies | 0.001 | 0.005 |
| Scholarly communication | 0.001 | 0.001 |
| Open science | 0.003 | 0.000 |
| Research integrity | 0.001 | 0.002 |
| Insufficient payload (model declined to judge) | 0.000 | 0.000 |
Machine scores (provisional)
The two teacher heads of the student model, read on this work. A score orders the frame for review; it never asserts a category, and the validation status ships verbatim with every row.
Baseline scores from an immature model (maturity gate not passed, 7 training rounds). Scores rank; they never assert a category.
score_only:v0-immature-baseline · verbatim from the scoring run: score_only means the number may rank works, and no category label ships from it